KR20150021271A - Ppg-chitosan hydrogel mask sheet comprising esculin and method for preparing the same - Google Patents

Abstract

The present invention relates to a PPG-chitosan hydrogel mask sheet containing esculin as an active ingredient and to a method for manufacturing the porous PPG-chitosan hydrogel mask sheet using the esculin extracted and isolated form mugwort. The method for manufacturing the PPG-chitosan hydrogel mask sheet containing the esculin as an active ingredient comprises a step for preparing a PPG-chitosan solution by dispersing PPG-chitosan powder in an acetic acid solution and then stirring; a step for making a PPG-chitosan hydrogel mask sheet by using sodium bicarbonate and glutaraldehyde as cross-linking agents with the PPG-chitosan solution; a step for obtaining dried powder by washing and grinding mugwort and extracting a mugwort extract using an extractant and then filtering, concentrating, and vacuum drying the extract; a step for fractionating the dried powder using purified water and an ethyl acetate solution and then filtering; a step for preparing solid powder by vacuum concentrating the filtered solution; a step for obtaining an esculin fraction by dissolving the solid powder in ethanol and then passing through a filled chromatography; and a step for impregnating the PPG-chitosan hydrogel mask sheet with the esculin fraction. Therefore, the present invention prevents excess sebum production and has effects on skin soothing and acne control, and enhances skin soothing and moisturizing effects by the composition.

Description

FIELD OF THE INVENTION [0001] The present invention relates to a PPG-CHITOSAN HYDROGEL MASK SHEET COMPRISING ESCULIN AND METHOD FOR PREPARING THE SAME,

The present invention relates to a phy- phyzite-chitosan hydrogel mask sheet containing esculin as an active ingredient and a method for producing the same, and more particularly, to a method for producing a phy- phage-chitosan hydrogel mask sheet using esculin, Chitosan hydrogel mask sheet comprising esculin which is excellent in skin calming and acne suppressing effect by preventing the excessive production of sebum by producing a mask sheet and a process for producing the same.

In modern society, active oxygen is generated by ultraviolet rays and water pollution due to destruction of ozone layer, emission of exhaust gas and harmful chemical substances, etc., and this active oxygen pours into the human body and causes various side effects, Skin aging and so on.

In order to prevent or treat the skin diseases caused thereby and to improve the skin, various skin external agents such as sunscreen agents, skin aesthetic agents, and cosmetics have been widely used and developed. However, these existing external skin preparations are merely supplying moisture and nutrients to the skin, and thus they can not supply specialized products that are effective for preventing skin damage on the face.

In addition, efforts and studies have been actively carried out to provide an improvement effect on the facial skin, and a mask sheet having a face-shaped sheet has been developed and supplied. Such a cosmetic mask sheet is made by adding water or a lotion to a nonwoven fabric or adding an extract or the like known to be functional. Nonwovens, however, are made of synthetic polymers. When added with cosmetic lotions or functional extracts, they become stiff and feel bad. Further, in the case of a formulation in which the nonwoven fabric is soaked in an additive such as a cosmetic liquid to induce absorption of a continuous serum, adhesion to the skin is low and denaturation of cosmetic ingredients caused by exposure of the serum to air is difficult to avoid, There is a disadvantage that skin irritation is likely to occur due to high-concentration cosmetic ingredients coming into contact with the skin.

On the other hand, sebaceous glands refer to secretions from sebaceous glands in the skin. Liquid fats secreted from the sebaceous glands are discharged through hair follicles through hair follicles to prevent drying of the skin surface.

Abnormal overproduction of such sebum leads to sebum-related diseases. In addition to sebum production, there are a number of deterioration factors. In other words, when sebum is not discharged out of the pores due to the exfoliation of the pores, primary fine microfilms are formed. Due to the action of Propionibacterium acnes , an anaerobic skin homologue existing in the pores of the pores, chronic inflammatory diseases such as papules, pustules, The scarring will occur. As a result, acne is caused by various congenital factors such as excessive production of sebum, exaggeration of pores, and action of Propionibacterium acnes .

Acne occurs mainly in puberty men and women. Generally, when puberty, male hormone secretion is active in both men and women to stimulate the sebaceous glands on the side of the hair follicles. Thus, the direct cause of acne is sebaceous glands secreted from sebaceous glands. The sebaceous glands are developed during puberty, which is strongly influenced by male hormones, and causes excessive sebum secretion. Testosterone, a type of male hormone, is converted into dihydrotestosterone by the 5 alpha-reductase in the skin, which binds to the cell receptor and signals DNA. As a result, the cleavage of sebaceous cells increases and lipid biosynthetic enzymes are activated, resulting in increased secretion of sebum. In particular, sebaceous glands are formed in the central part of the body such as face, chest, and scalp, and sebum is produced in a large amount. When sebum is not properly discharged, sebum accumulates and consequently causes acne. (Note: Tahir Muhammad Ch, Pathogenesis of acne vulgaris, Journal of Pakistan Association of Dermatology, 20, 93-97, 2010)

When antibiotics such as tetracycline are used as antimicrobial substances against Propionibacterium acnes , there is a great possibility of causing adverse effects such as the appearance of resistant bacteria or the photosensitization. In most cases, hormone preparations, antibiotics, and oral medicines are used to treat acne, but excessive use or misuse can cause side effects such as skin irritation, contact dermatitis, dermatitis, and skin irritation.

Therefore, prevention is more important than acne treatment. One such prophylactic method is sebum control. BACKGROUND ART [0002] Benzoyl peroxide and salicylic acid are widely known as healing ingredients of acne in the past. (Reference: Ha, Byung Jo, Cosmetology, 91-93, 2010,

Benzoyl peroxide is used at a rate of 2.5 ~ 10%, which has side effects of itching and burning. Salicylic acid is used in a ratio of 0.5 ~ 2%, and since it is poor in water solubility, precipitates often form at low temperature and it is usually formulated with ethanol.

However, these formulations tend to dry quickly due to the evaporation of alcohol, and also generally people want to feel moist with calm when using acne products, evaporation of alcohol makes the skin dry. In addition, there is a problem that excessive exfoliation is caused at a high concentration and skin irritation is caused.

Korean Patent Laid-Open No. 10-2008-0055131 (published on June 13, 2008) Domestic Registration No. 10-1240254 (Registered on February 28, 2013) Korean Patent Laid-Open No. 10-2011-0054224 (published on May 25, 2011) Korean Patent Publication No. 10-2013-0036543 (published on April 12, 2013)

It is an object of the present invention to overcome the above-mentioned problems, and it is an object of the present invention to provide a porous structure-based phyphosis-chitosan hydrogel mask sheet using esculin extracted from mugwort to prevent excessive production of sebum, Chitosan hydrogel mask sheet containing esculin as an effective ingredient.

In addition, the present invention relates to a pharmaceutical composition comprising a porous phypho-chitosan hydrogel sheet, which is capable of reducing adverse effects of active ingredients of acne and enhancing skin soothing and moisturizing action, Sheet.

In addition, the present invention can be applied to the production of a hydrogel mask sheet in which phyphage-chitosan, which improves the disadvantages of chitosan which can be discolored by reactive amino groups or cause skin side effects, Chitosan hydrogel mask sheet comprising esculin as an active ingredient which can be simultaneously alleviated.

The various problems to be solved by the present invention are not limited to the above-mentioned problems, and other problems not mentioned can be clearly understood by those skilled in the art from the following description.

The method for producing a phy- phage-chitosan hydrogel mask sheet comprising esculin according to the present invention as an active ingredient comprises the steps of dispersing phy- phyzate-chitosan powder in an acetic acid solution and then stirring to prepare a phy- phage-chitosan solution; Preparing a phy- phzi-chitosan hydrogel mask sheet by using sodium bicarbonate and glutaraldehyde as a crosslinking agent in the phy- phyzate-chitosan solution; Washing the wormwood leaves and pulverizing them, filtering and concentrating and vacuum-drying the raw stock solution with an extraction solvent to obtain a dry powder; Separating the dried powder into purified water and ethyl acetate solution and then filtering; Concentrating the filtered solution in vacuo to produce a solid powder; Dissolving the solid powder in ethanol and passing it through packed chromatography to obtain an esculin fraction; And impregnating the phyphage-chitosan hydrogel mask sheet with the esculin fraction.

The step of dispersing the phyphage-chitosan powder in the acetic acid solution followed by stirring to prepare the phyphage-chitosan solution is carried out by dispersing the phyphage-chitosan powder in a 0.5% acetic acid solution while maintaining the room temperature, Solution. ≪ / RTI >

The step of preparing the phy- phage-chitosan hydrogel mask sheet using the sodium bicarbonate and the glutaraldehyde as a crosslinking agent in the phy- phyzate-chitosan solution may be carried out by adding a phy- phyzate-chitosan solution in which powdery sodium bicarbonate has been completely de- Mixing the carbon dioxide gas to generate carbon dioxide gas; Adding glutaraldehyde to the mixed solution to prepare a mask sheet; And washing the mask sheet with purified water followed by lyophilization to prepare a phy- phyzate-chitosan hydrogel mask sheet.

The PHJ-chitosan hydrogel mask sheet may be formed in the form of a porous sponge.

The step of washing the wormwood leaves and pulverizing and extracting the extract solution with an extraction solvent, filtrating, concentrating and vacuum drying the extract to obtain a dry powder can use 75% ethanol as an extraction solvent.

The step of separating the dried powder into purified water and ethyl acetate solution followed by filtration may use a solution prepared by mixing the purified water with ethyl acetate in a ratio of 1: 1.

The step of fractionating the dried powder with purified water and ethyl acetate solution followed by filtration may include fractionating with ethyl acetate solution, adding anhydrous magnesium sulfate for dehydration, and then filtering.

In addition, the present invention may include a phy- phyzate-chitosan hydrogel mask sheet containing esculin as an active ingredient, which is produced by the above-described production method.

The details of other embodiments are included in the detailed description and drawings.

The phy- phyzate-chitosan hydrogel mask sheet comprising esculin according to the present invention as an effective ingredient has an effect of preventing excessive production of sebum and excellent in skin soothing and acne suppressing effect.

Further, the phy- phyzate-chitosan hydrogel mask sheet comprising esculin according to the present invention as an active ingredient has the effect of reducing the side effects of acne-active ingredients and increasing skin soothing and moisturizing action.

The process for producing a phy- phyzate-chitosan hydrogel mask sheet comprising esculin according to the present invention as an active ingredient has the disadvantages of chitosan which can be discolored due to reactive amino groups or cause skin side effects, So that it is possible to simultaneously alleviate discoloration and skin side effects.

It will be appreciated that embodiments of the technical idea of the present invention can provide various effects not specifically mentioned.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is an optical microscope photograph of a porous fibrous chitosan sheet according to Example 1 of the present invention. FIG.
2 is an electron micrograph of a porous particulate-chitosan sheet according to Example 1 of the present invention.
3 is a graph showing the FR-IR spectrum of the dried powder after extraction with 75% ethanol in Example 2 according to the present invention.
4 is a photograph showing a separation experiment of Sephadex LH-20 in Example 2 according to the present invention.
Figure 5 is a photograph showing the TLC of the fraction containing esculin in Example 2 according to the present invention.
Figure 6 is a diagram showing the UV spectrum of the fraction containing esculin in Example 2 according to the present invention.
Figure 7 is an LC-MASS spectrum of a fraction containing esculin in Example 2 according to the present invention.
FIG. 8 is a photograph showing the results of an E. coli antimicrobial test of a 75% ethanol extract of Mugwort plant extract in Example 3 according to the present invention. FIG.
9 is a photograph showing the results of an Escherichia coli antibacterial test in Example 3 according to the present invention.
10 is a photograph showing the results of S. aureus antimicrobial test on 75% ethanol extract of mugwort extract in Example 3 according to the present invention.
11 is a photograph showing the results of S. aureus antibacterial test of esculin in Example 3 according to the present invention.
12 is a photograph showing the results of the antibacterial activity against P. acnes of the extract solution of mugwort 75% ethanol extract in Example 3 according to the present invention.
13 is a photograph showing the results of antibacterial activity against P. acnes in Escherichia in Example 3 according to the present invention.

BRIEF DESCRIPTION OF THE DRAWINGS The advantages and features of the present invention, and how to accomplish them, will become apparent by reference to the embodiments described in detail below with reference to the accompanying drawings. However, the present invention is not limited to the embodiments described herein but may be embodied in other forms. Rather, the embodiments disclosed herein are provided so that the disclosure can be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.

The terminology used in this application is used only to describe a specific embodiment and is not intended to limit the invention. The singular expressions include plural expressions unless the context clearly dictates otherwise. In this application, the terms "comprises", "having", and the like are used to specify that a feature, a number, a step, an operation, an element, a part or a combination thereof is described in the specification, But do not preclude the presence or addition of one or more other features, integers, steps, operations, components, parts, or combinations thereof.

Unless otherwise defined, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Terms such as those defined in commonly used dictionaries are to be interpreted as having a meaning consistent with the meaning in the context of the relevant art and are to be construed as ideal or overly formal in meaning unless explicitly defined in the present application Do not.

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings, in which a phy- phyzate-chitosan hydrogel mask sheet comprising esculin as an active ingredient and a method for producing the same.

Esculin used in the present invention is a compound having a chemical structure such as the following formula 1, and the chemical name of esculin is 7-hydroxycoumarin-6-yl-β-D-glucoside. The esculin can be synthesized by a chemical method or extracted from mugwort as a known compound. In the technical aspects of the present invention, the esculin includes those extracted from mugwort.

[Chemical Formula 1]. Chemical structure of esculin

Example 1 Preparation of Porous Phyji-Chitosan Sheet

While maintaining the room temperature at 1 liter of a 0.5% acetic acid solution, the phyphage-chitosan powder is slowly dispersed in small portions and stirred. After stirring, the undissolved phyphage-chitosan is removed by filtration to prepare a 1% phyphage-chitosan solution, and the bubbles in the solution are defoamed and removed.

1 g of powdered sodium bicarbonate was spread evenly on the bottom of a polyethylene shale having a diameter of 20 cm, and 20 g of a phy- phage-chitosan solution having been completely deaerated was added, and carbon dioxide gas was generated so that air bubbles were uniformly generated in the liquid.

After mixing for 3 minutes at 400 rpm, 1 ml of glutaraldehyde (25%) was added dropwise. After the sample was left to stand for 24 hours, 20 ml of 10% sodium hydroxide was added and left for 30 minutes. Then, the sample was removed from the container through aqueous solution and solvent exchange, washed several times with purified water and lyophilized to form a sponge- To obtain porous porous paper-chitosan sheet. The optical microscope photograph of the porous paper-chitosan sheet is shown in FIG. 1, and the electron micrograph of the porous paper-chitosan sheet is as shown in FIG.

Example 2 Extraction of Esculin from Mugwort

The wormwood was washed and powdered, and then cooled with 10 times of extraction solvent (75% ethanol) at room temperature for 5 days. Then, the extract solution was filtered, concentrated and vacuum dried to obtain a dry powder. The FR-IR spectrum of the dried powder after extraction with 75% ethanol is as shown in FIG. The fraction was further subjected to three times of addition of a purified water: ethyl acetate (1: 1) solution. Ethyl acetate layer was obtained, dried over anhydrous magnesium sulfate for dehydration and filtered.

The filtrate was concentrated in vacuo to obtain a brown solid powder. After dissolving in 95% ethanol, the product was passed through chromatography packed with Sephadex LH-20 to obtain pure esculine fraction. 4, the TLC of the fraction containing Esculin is shown in FIG. 5, and the UV spectrum of the fraction containing Esculin is shown in FIG. 6 And the LC-MASS spectrum of the fraction containing esculin is as shown in FIG.

Example 3. Measurement of antibacterial effect of esculin

The antimicrobial activity of Escherichia coli, Staphylococcus aureus, and Acne bacteria purified from 75% ethanol extract of mugwort and purified Escherichia coli was tested by Halo test against Escherichia coli, Staphylococcus aureus and Acne bacteria. Respectively.

First, Escherichia coli and Staphylococcus aureus were inoculated into a liquid medium (Brain heart infusion broth) and enriched for 24 hours at 35 ° C. The acne bacteria were inoculated on Fluid Thioglycolate Medium medium 0.0 > C < / RTI > for 72 hours. The extract solution of 75% ethanol extract was used as it was without dilution, and esculin was prepared by using 10% (w / v) solution of DMSO as a solvent. The back aliquots of E. coli and S. aureus were inoculated evenly on sterile swabs to trytic soy agar plate media. Approximately 17 mg of the sample was treated with a sterilized paper disk (Ø6.0), and 13 μl of a 10% (w / v) solution of the extract was applied to a paper disk, and each paper disk was placed in the center of the medium. This was incubated at 35 DEG C for 24 hours to measure the inhibition zone formed. For P. acnes, the bacterial culture was inoculated evenly on a Brewer's Anaerobic Agar plate medium with a sterile cotton swab.

Approximately 17 mg of 75% ethanol extract concentrate was applied to a sterilized paper disk (Ø6.0) in the same manner as above, and 13 μl of 10% (w / v) Was placed in the center of the medium. After incubation in an anaerobic jar at 35 ° C for 72 hours under aerobic conditions, the diameter of the low-lying zone was measured.

The size of the lowland W = (T-D) / 2

Where W is the size of the low zone (mm), T is the total length (mm) of the sample and the low zone, and D is the length of the sample (mm).

The following results were obtained.

1) Results of E. coli antibacterial test Sample classification T D W 75% ethanol extract of mugwort extract 6 6 0 Esculin 10 6 2

The photograph of the result of the E. coli antibacterial test of 75% ethanol extract of Mugwort is shown in FIG. 8, and the photograph of the result of Escherichia coli antibacterial test is as shown in FIG.

2) Results of S. aureus antibacterial test Sample classification T D W 75% ethanol extract of mugwort extract 6 6 0 Esculin 16 6 5

Fig. 10 shows photographs of S. aureus antibacterial test results of 75% ethanol extract of mugwort, and Fig. 11 shows photographs of S. aureus antibacterial test results of Escherichia.

3) Results of P. acnes antibacterial test Sample classification T D W 75% ethanol extract of mugwort extract 6 6 0 Esculin 14 6 4

The results of the P. acnes antibacterial test on the 75% ethanol extract of Mugwupi extract are shown in FIG. 12, and the photograph of the result of the antibacterial test on P. acnes of Esculin is shown in FIG.

While the present invention has been described in connection with what is presently considered to be practical exemplary embodiments, it is to be understood that the invention is not limited to the disclosed embodiments, but, on the contrary, It will be understood that the invention may be practiced. It is therefore to be understood that one embodiment described above is illustrative in all aspects and not restrictive.

Claims (8)

Dispersing phyphage-chitosan powder in an acetic acid solution and stirring the phyphage-chitosan powder to prepare a phy- phyzate-chitosan solution;
Preparing a phy- phzi-chitosan hydrogel mask sheet by using sodium bicarbonate and glutaraldehyde as a crosslinking agent in the phy- phyzate-chitosan solution;
Washing the wormwood leaves and pulverizing them, filtering and concentrating and vacuum-drying the raw stock solution with an extraction solvent to obtain a dry powder;
Separating the dried powder into purified water and ethyl acetate solution and then filtering;
Concentrating the filtered solution in vacuo to produce a solid powder;
Dissolving the solid powder in ethanol and passing it through packed chromatography to obtain an esculin fraction; And
And a step of impregnating the phy- phyzite-chitosan hydrogel mask sheet with the esculin fraction. The method of producing a phy- phyzate-chitosan hydrogel mask sheet comprising esculin as an active ingredient.
The method according to claim 1,
The step of dispersing the phyphage-chitosan powder in the acetic acid solution followed by stirring to prepare the phyphage-chitosan solution is carried out by dispersing the phyphage-chitosan powder in a 0.5% acetic acid solution while maintaining the room temperature, The method of producing a phy- phyzite-chitosan hydrogel mask sheet comprising esculin as an active ingredient, characterized in that it is a step of producing a solution.
The method according to claim 1,
The step of preparing a phy- phyzate-chitosan hydrogel mask sheet using sodium bicarbonate and glutaraldehyde as a cross-linking agent in the phy-
Adding a phage-chitosan solution in which the de-posed phage-chitosan solution is added to powdered sodium bicarbonate, and mixing the resultant to generate carbon dioxide gas;
Adding glutaraldehyde to the mixed solution to prepare a mask sheet; And
Wherein the mask sheet is washed with purified water and then lyophilized to prepare a phy- phyzate-chitosan hydrogel mask sheet. The method for producing a mask for phy- chi-chitosan hydrogel mask according to claim 1,
The method of claim 3,
Wherein the phy- phyzite-chitosan hydrogel mask sheet is formed in the form of a porous sponge.
The method according to claim 1,
The step of washing and drying the wormwood leaves to obtain a dry powder by filtration, concentration and vacuum drying of the extractive liquid with an extraction solvent is characterized in that 75% ethanol is used as an extraction solvent, A process for producing a chitosan hydrogel mask sheet.
The method according to claim 1,
The step of fractionating the dried powder with purified water and ethyl acetate solution followed by filtration is carried out by using a solution prepared by mixing the purified water with ethyl acetate in a ratio of 1: 1. A method for producing a hydrogel mask sheet.
The method according to claim 1,
The step of fractionating the dried powder with purified water and ethyl acetate solution followed by filtration is carried out by fractionating with ethyl acetate solution, adding anhydrous gum for dehydration, and then filtering. A method for producing a sebum-chitosan hydrogel mask sheet.
A phy- phyzite-chitosan hydrogel mask sheet comprising esculin as an active ingredient, which is produced by the production method of any one of claims 1 to 7.

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